CN113801144B - X-ray excited luminescent material and preparation method thereof - Google Patents

X-ray excited luminescent material and preparation method thereof Download PDF

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CN113801144B
CN113801144B CN202111224149.4A CN202111224149A CN113801144B CN 113801144 B CN113801144 B CN 113801144B CN 202111224149 A CN202111224149 A CN 202111224149A CN 113801144 B CN113801144 B CN 113801144B
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刘湘梅
姜阳阳
陶小芳
赵强
刘淑娟
黄维
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Nanjing University of Posts and Telecommunications
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Abstract

The invention discloses an X-ray excitation luminescent material and a preparation method thereof, wherein the crystal luminescent material takes cuprous iodide or cuprous bromide as a core and takes 3-Complexes of picolines and triphenylphosphine as ligands, i.e. CuI (Pph) which emits a strong fluorescence under X-ray or UV excitation 3 ) 2 (3-pc) or CuBr (Pph) 3 ) 2 The (3-pc) two complexes have excellent ultraviolet and X-ray luminescence properties and higher quantum efficiency. The X-ray excited luminescent crystal has the advantages of simple preparation steps, short time consumption, high luminous efficiency and the like, and therefore has important application prospects in the aspects of biological imaging, photodynamic therapy, X-ray imaging and the like.

Description

X-ray excited luminescent material and preparation method thereof
Technical Field
The invention belongs to the technical field of X-ray excited scintillation materials and luminescent crystal materials, and particularly relates to an X-ray excited luminescent material and a preparation method thereof.
Background
The X-ray scintillating luminescent material is widely applied and is basically characterized in that the X-ray scintillating luminescent material can receive high-energy particle beams of X-rays and convert ionizing radiation of the X-rays into photon energy of visible light, and the X-ray scintillating luminescent material is applied to the aspects of medical imaging, radiation monitoring, safety inspection, cancer diagnosis, photodynamic therapy and the like due to high penetrability of the X-rays. Although the high penetration of X-rays gives scintillating materials advantages for various applications in various fields, it also leads to significant disadvantages of the X-ray scintillating materials themselves. The propagation path of visible light or near infrared light is immediately cut off when the visible light or the near infrared light is shielded by a solid object in the propagation process, the energy of the visible light or the near infrared light is greatly reduced when the visible light or the near infrared light passes through a transparent object, the X-ray is different from general visible light, the X-ray has high penetrability in most metals in the propagation process, the propagation depth in biological tissues is not limited, and the energy carried by the X-ray is far higher than that of the visible light. Compared with luminescent materials under ultraviolet conditions, the X-ray scintillator is more applied to nondestructive detection of various information inside an object and luminescent imaging in the deep tissue. Since the high permeability of X-rays leads to a smaller inventory of materials in nature and synthesized in laboratory conditions compared to luminescent materials under uv conditions, and in addition, the high permeability of X-rays also leads to a lower energy utilization of the scintillating luminescent material for X-rays, the importance of developing a new type of X-ray scintillating material is self-evident.
Based on the wide application and importance of the X-ray scintillation luminescent material, many research teams have conducted many beneficial explorations on X-ray scintillators, and are dedicated to finding new materials with high energy conversion efficiency and exploring simple methods for controlling crystal production so as to prepare the X-ray scintillation luminescent material with high Z value, high quantum yield, excellent energy resolution, large-scale preparation and low cost. Representative materials include doping of various inorganic halides with Tl 2 LiGdCl 6 : Ce 3+ 、Tl 2 LiYCl 6 : Ce 3+ 、Tl 2 LaBr 5 : Ce 3+ Metal oxide CaWO 4 、Bi 4 Ge 3 O 12 、BaWO 2 F 4 Halogenated perovskite CsPbBr 3 、Rb 2 CuBr 3 、Cs 2 NaTbCl 6 The materials can achieve ideal effects in practical application by detecting various properties, and are widely applied to the aspects of homeland security, nuclear physics experiments, radioactive pollution detection and the like. Most of the scintillation crystals are prepared under a high-temperature condition, the preparation condition is relatively harsh, the requirement on experimental calcination equipment is relatively high, although experimental improvement finds that the environmental requirement on perovskite reaction experiment is reduced, the scintillation crystals can be obtained by adopting hydrothermal, solution precipitation, vacuum precipitation and other modes, the requirement on temperature is greatly reduced, and the obtained scintillation material still faces the problems of containing heavy metal elements and toxic metals, complex preparation method, less material selection range, randomness in light-emitting wavelength and the like.
Therefore, in order to expand the types of X-ray scintillators, simplify experimental methods, reduce the number of protons of material metals and regulate and control the luminescent wavelength of materials, small-molecule complexes taking cuprous halide as a core 3-methylpyridine and triphenylphosphine as ligands are researched through experiments, the small-molecule complexes have excellent luminescent properties under ultraviolet and X-ray conditions, the materials have extremely high photoluminescence quantum efficiency, and are expected to be well applied in the fields of X-ray luminescent display materials and the like, so that the small-molecule complexes have very important research significance.
Disclosure of Invention
In order to solve the above problems, the present invention provides an X-ray excited luminescent material and a method for preparing the same. A perfect crystal is obtained by controlling experimental conditions, and the crystal has extremely high luminous quantum efficiency, so that the material has good application prospects in the aspects of biological imaging, photodynamic therapy, X-ray imaging and the like.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the invention relates to an X-ray excitation luminescent material, which takes cuprous iodide or cuprous bromide as a core, 3-methylpyridine (3-pc) and triphenylphosphine (Pph) 3 ) Complexes being ligands, i.e. CuI (Pph) emitting intense fluorescence under X-ray or UV excitation 3 ) 2 (3-pc) and CuBr (Pph) 3 ) 2 (3-pc) two complexes, cuI (Pph) 3 ) 2 The structural formula of the (3-pc) complex is as follows:
Figure 467602DEST_PATH_IMAGE002
；
the CuBr (Pph) 3 ) 2 The structural formula of the (3-pc) complex is as follows:
Figure 853584DEST_PATH_IMAGE004
。
the invention is further improved in that: the CuI (Pph) 3 ) 2 The emission band of (3-pc) is 400-650 nm, and the emission peak is 467 nm.
The invention is further improved in that: cuBr (Pph) 3 ) 2 The emission band of (3-pc) is 400-650 nm, and the emission peak is 500 nm.
A preparation method of an X-ray excitation luminescent material comprises the following specific synthetic lines:
Figure 102163DEST_PATH_IMAGE006
wherein CuX is cuprous iodide or cuprous bromide, cu 2 X 2 (3-pc) 4 Is Cu 2 I 2 (3-pc) 4 Or Cu 2 Br 2 (3-pc) 4 ，CuX(Pph 3 ) 2 (3-pc) is CuI (Pph) 3 ) 2 (3-pc) or CuBr (Pph) 3 ) 2 (3-pc) 。
The invention is further improved in that: the preparation steps are as follows:
step 1, cu 2 X 2 (3-pc) 4 The preparation of (1):
firstly, cuprous halide is fully dispersed in an open reaction bottle in acetone to form a suspension, 3-pc is slowly added under magnetic stirring at room temperature, the continuous stirring reaction is carried out for a period of time, and the suspension is changed into a clear and transparent solution;
step 2, cuX (Pph) 3 ) 2 Preparation of (3-pc):
taking the Cu obtained in the step 1 2 X 2 (3-pc) 4 Adding acetone to dilute the solution to a certain concentration range, dissolving triphenylphosphine in toluene, and adding diluted Cu 2 X 2 (3-pc) 4 Slightly shaking the acetone solution to uniformly mix the acetone solution and the acetone solution;
step 3, crystal growth:
and sealing and standing the solution after uniform oscillation to crystallize the solution, and collecting crystals after 24 hours.
The invention is further improved in that: cuI (Pph) prepared in step 3 3 ) 2 (3-pc) or CuBr (Pph) 3 ) 2 The (3-pc) crystal is a colorless blocky crystal, can be stably stored at the temperature of 100 ℃, and has a structure in a monodentate form.
The invention is further improved in that: cu in step 2 2 X 2 (3-pc) 4 The concentration of the acetone solution of (1) is 0.01 mmol/mL to 0.10 mmol/mL.
The invention is further improved in that: the ratio of reactant ligands is Pph 3 ：(3-pc) =2:1 to Pph 3 ：(3-pc)=3：1。
The invention has the beneficial effects that: the luminescent material is a cuprous halide complex prepared by a two-step method, and is Cu 2 X 2 (3-pc) 4 For the primary product, a new complex is formed by adding triphenylphosphine to replace the original ligand, and CuI (Pph) is obtained based on different halogens, namely iodine element and bromine element 3 ) 2 (3-pc) with CuBr (Pph) 3 ) 2 (3-pc), and the obtained crystal can emit strong fluorescence under the excitation of X rays or ultraviolet light. The method has the advantages of simple experimental operation steps, perfect crystal growth, ultrahigh luminescent quantum efficiency under ultraviolet excitation and excellent X-ray excitation luminescent performance. The raw materials are rich and easy to obtain, the application range is wide, and the method is favorable for further research.
Drawings
FIG. 1 shows an X-ray excited luminescent material CuI (pph) prepared in example 3 3 ) 2 (3-pc) Crystal Structure of a single molecule.
FIG. 2 shows an X-ray excited luminescent material CuI (pph) prepared in example 3 3 ) 2 Unit cell arrangement diagram of (3-pc).
FIG. 3 shows a sample of an X-ray excited luminescent material CuBr (pph) prepared in example 5 3 ) 2 (3-pc) Crystal Structure of a single molecule.
FIG. 4 shows a sample of an X-ray excited luminescent material CuBr (pph) prepared in example 5 3 ) 2 Unit cell arrangement diagram of (3-pc).
FIG. 5 is an X-ray excited scintillation crystal CuI (pph) prepared in example 4 3 ) 2 Excitation spectrum of (3-pc) and emission spectrum under optimum excitation.
FIG. 6 is an X-ray excited scintillation crystal CuBr (pph) prepared in example 5 3 ) 2 Excitation spectrum of (3-pc) and emission spectrum under optimum excitation.
FIG. 7 shows an X-ray excited luminescent material CuI (tpp) prepared in example 1 2 (3-pc) and CuBr (tpp) prepared in example 2 2 (3-pc) ultraviolet excited emission spectrum.
FIG. 8 shows an X-ray excited luminescent material CuBr (tpp) prepared in example 2 2 (3-pc) and CuI (tpp) prepared in example 1 2 (3-pc) X-ray excitation emission spectrum.
Table 1 shows X-ray excited luminescent materials CuI (pph) 3 ) 2 (3-pc)、CuBr(pph 3 ) 2 Average interatomic distance of (3-pc).
Table 2 shows the comparison of the normal temperature and 77K low temperature life time of two complexes of X-ray excited luminescent materials and the luminescent quantum efficiency thereof under ultraviolet excitation.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the present invention more readily understandable to those skilled in the art, and will thus provide a more clear and concise definition of the scope of the appended claims. These examples are illustrative only and are not to be construed as limiting the invention since they are intended to be specifically described herein.
The X-ray excitation luminescent material takes cuprous halide (CuX) as a core, 3-methylpyridine (3-pc) and triphenylphosphine (Pph) 3 ) Is a complex of ligand, wherein CuX can be CuI or CuBr, and the crystal luminescent material is CuI (Pph) 3 ) 2 (3-pc) or CuBr (Pph) 3 ) 2 (3-pc)。CuI(Pph 3 ) 2 (3-pc) and CuBr (Pph) 3 ) 2 (3-pc) are all colorless blocky crystals which can be stably stored at 100 ℃, and the crystal luminescent material is subjected to X-ray single crystal diffraction test and the structure of the crystal luminescent material is analyzed, so that the crystal is not a cluster-shaped structure of a conventional CuX complex but is in a form of single coordination; can emit strong fluorescence under the excitation of X rays or ultraviolet light, wherein, cuI (Pph) 3 ) 2 The emission band of (3-pc) is 400-650 nm, and the emission peak is 467 nm; cuBr (Pph) 3 ) 2 The emission band of (3-pc) is 400-650 nm, and the emission peak is 500 nm.
The preparation method of the X-ray excitation luminescent material comprises the following steps:
example 1
Step 1, cu 2 I 2 (3-pc) 4 The preparation of (1):
first, cuprous iodide (1.0 mmol) was well dispersed in a 10mL open reaction flask in acetone to form a suspension, and 3-methylpyridine (4.0 mmol) was slowly added under magnetic stirring at room temperature, and after stirring for a while, the suspension reacted to a clear solution.
Step 2, cuI (Pph) 3 ) 2 Preparation of (3-pc):
2 ml of reacted Cu were taken 2 I 2 (3-pc) 4 Solution triphenylphosphine (0.5 mmol) dissolved in 2 ml toluene and Cu added 2 I 2 (3-pc) 4 In acetone solution, lightly shaking to mix them uniformly, wherein, cu 2 I 2 (3-pc) 4 The concentration of the acetone solution of (1) is 0.01 mmol/mL to 0.10 mmol/mL.
Step 3, crystal growth:
and sealing and standing the solution after uniform oscillation to crystallize the solution, and collecting crystals after 24 hours.
Example 2
Step 1, cu 2 Br 2 (3-pc) 4 The preparation of (1):
first, cuprous bromide (1.0 mmol) was well dispersed in a 10mL open reaction flask in acetone to form a suspension, and 3-pc (4.0 mmol) was slowly added under magnetic stirring at room temperature. After a period of continuous stirring, the suspension reacts to a clear solution.
Step 2, cuBr (Pph) 3 ) 2 Preparation of (3-pc):
2 ml of reacted Cu were taken 2 Br 2 (3-pc) 4 Solution triphenylphosphine (0.5 mmol) dissolved in 2 ml toluene and Cu added 2 Br 2 (3-pc) 4 The mixture was gently shaken to mix the mixture uniformly. Wherein, cu 2 Br 2 (3-pc) 4 The concentration of the acetone solution of (1) is 0.01 mmol/mL to 0.10 mmol/mL.
Step 3, crystal growth:
and sealing and standing the solution after uniform oscillation to crystallize the solution, and collecting crystals after 24 hours.
Example 3
Step 1, cu 2 I 2 (3-pc) 4 The preparation of (1):
firstly, fully dispersing cuprous iodide (1.0 mmol) in an open reaction bottle of 10mL acetone to form a suspension, dropwise adding a small amount of saturated KI solution into the suspension to completely dissolve the cuprous iodide, slowly adding 3-pc (4.0 mmol) under magnetic stirring at room temperature, and continuously stirring for 10min to gradually clarify the suspension.
Step 2, cuI (Pph) 3 ) 2 Preparation of (3-pc):
crystallizing the solution in (1) to obtain Cu 2 I 2 (3-pc) 4 0.15 g of the needle-like crystals of (3) were dissolved in 10ml of acetone, triphenylphosphine (0.5 mmol) was dissolved in 2 ml of toluene, and dissolved Cu was added 2 I 2 (3-pc) 4 The mixture was gently shaken to mix the mixture uniformly.
Step 3, crystal growth:
and sealing and standing the solution after uniform oscillation to crystallize the solution, and collecting crystals after 24 hours.
Example 4
CuI(Pph 3 ) 2 (3-pc)
Step 1, cu 2 I 2 (3-pc) 4 The preparation of (1):
first, cuprous iodide (1 mmol) was well dispersed in a 5mL acetone in an open reaction flask to form a suspension, and 3-pc (4 mmol) was slowly added under magnetic stirring at room temperature, and after stirring for 10min continuously, the solution became clear.
Step 2, cuI (Pph) 3 ) 2 Preparation of (3-pc):
2 ml of reacted Cu were taken 2 I 2 (3-pc) 4 The solution was diluted to 1/20 of the original concentration with acetone. Triphenylphosphine (1 mmol) was dissolved in 10ml toluene and diluted Cu was added 2 I 2 (3-pc) 4 The mixture was gently shaken to mix the mixture uniformly.
Step 3, crystal growth:
and sealing and standing the solution after uniform oscillation to crystallize the solution, and collecting crystals after 24 hours.
Example 5
CuBr(Pph 3 ) 2 (3-pc)
Step 1, cu 2 Br 2 (3-pc) 4 The preparation of (1):
first, cuprous bromide (1 mmol) was well dispersed in 5mL acetone in an open reaction flask to form a suspension, 3-pc (4 mmol) was slowly added under magnetic stirring at room temperature, and after stirring for 10min continuously, solution step 2, cuBr (Pph) 3 ) 2 Preparation of (3-pc):
2 ml of reacted Cu were taken 2 Br 2 (3-pc) 4 The solution was diluted to 1/20 of the original concentration with acetone. Triphenylphosphine (5 mmol) was dissolved in 2 ml toluene and diluted Cu was added 2 Br 2 (3-pc) 4 The mixture was gently shaken to mix the mixture uniformly.
Step 3, crystal growth:
and sealing and standing the solution after uniform oscillation to crystallize the solution, and collecting crystals after 24 hours.
The X-ray excited luminescent material prepared in the embodiments 1 to 5 has excellent ultraviolet and X-ray luminescent properties, has high quantum efficiency, is simple in preparation steps and short in time, and has important application prospects in aspects of biological imaging, photodynamic therapy, X-ray imaging and the like.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.

Claims (1)

1. Structural formula is
Figure DEST_PATH_IMAGE001
The complex CuI (Pph) of (1) 3 ) 2 (3-pc) and the structural formula
Figure 372309DEST_PATH_IMAGE002
The complex CuBr (Pph) 3 ) 2 (3-pc) in X-ray excited luminescent materials.
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